CN113840400A - Heater and preparation method thereof - Google Patents

Heater and preparation method thereof Download PDF

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Publication number
CN113840400A
CN113840400A CN202111061001.3A CN202111061001A CN113840400A CN 113840400 A CN113840400 A CN 113840400A CN 202111061001 A CN202111061001 A CN 202111061001A CN 113840400 A CN113840400 A CN 113840400A
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graphene
conductor
heating cavity
electrode layer
heating
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宋琪
姜斌
王惠明
李涅
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Raytheon New Materials Suzhou Co ltd
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Raytheon New Materials Suzhou Co ltd
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    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B3/00—Ohmic-resistance heating
    • H05B3/02—Details
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B3/00—Ohmic-resistance heating
    • H05B3/02—Details
    • H05B3/04—Waterproof or air-tight seals for heaters
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B3/00—Ohmic-resistance heating
    • H05B3/10—Heater elements characterised by the composition or nature of the materials or by the arrangement of the conductor
    • H05B3/12—Heater elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material
    • H05B3/14—Heater elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material the material being non-metallic
    • H05B3/145—Carbon only, e.g. carbon black, graphite

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Abstract

The invention belongs to the technical field of heating elements, and relates to a heater and a preparation method thereof. The heater and the preparation method thereof provided by the invention have the advantages that the effect of rapid and uniform heating is realized, no limitation is caused to the shape of the heating cavity, and no obvious requirement is caused on the mechanical strength of the graphene conducting layer. The graphene conducting layer in the heater can resist the high temperature of 800 plus 1100 ℃, the working temperature reaches 800 ℃, the heating life is longer than 30000h, and the heating time is more than 20W/cm2The power density of (d); heating simultaneouslyThe waterproof and insulating device has good waterproof and insulating properties.

Description

Heater and preparation method thereof
Technical Field
The invention belongs to the technical field of heating elements, and particularly relates to a heater and a preparation method thereof.
Background
Graphene is a polymer made of carbon atoms in sp2The hybrid tracks form a hexagonal honeycomb lattice planar film, the two-dimensional material with the thickness of only one carbon atom is the thinnest nano material, the two-dimensional honeycomb lattice planar film is almost completely transparent and only absorbs 2.3% of light, the heat conductivity coefficient of the graphene is higher than that of the carbon nano tubes and the diamond, the electron mobility at normal temperature is higher than that of the carbon nano tubes or the silicon crystal, and the resistivity is lower than that of copper or silver. The graphene has excellent electrothermal conversion efficiency and electrothermal radiation conversion efficiency. After being electrified, the graphene can efficiently convert electric energy into heat energy and radiate the heat energy out through far infrared rays, so that the graphene is an ideal electric heating material. However, the graphene has an obvious oxidation process at 500 ℃, and the resistance is increased continuously, so that the power is attenuated continuously; therefore, graphene-based heating products cannot achieve power density>2W/cm2And the long-time electrifying heating at the temperature higher than 500 ℃ limits the application range of the graphene heating product. Meanwhile, the mechanical strength requirement of the graphene heating structure in the existing graphene heating product is high due to the graphene heating structure, the heating speed is low, the high-temperature surface insulation and packaging of the heater are difficult to realize, and good waterproof performance and insulating performance cannot be realized.
Disclosure of Invention
The invention aims to solve the technical problems that the existing graphene heating product cannot realize long-time heating at the temperature higher than 500 ℃, the mechanical strength requirement of a graphene heating element is high, the heating speed is low, and good waterproof performance and insulating performance cannot be realized.
In order to solve the above technical problems, in one aspect, the present invention provides a heater, including a heating cavity, a graphene conductive layer, a first conductor, and a second conductor, where the graphene conductive layer is attached to an inner wall of the heating cavity, the first conductor and the second conductor are electrically connected to different positions of the graphene conductive layer, respectively, the first conductor and the second conductor extend to an outside of the heating cavity, and the heating cavity is a sealing structure.
Preferably, the first conductor and the second conductor extend to the outside of the heating cavity and are arranged on two sides of the heating cavity or on the same side of the heating cavity; the interior of the heating cavity is in a vacuum state or is filled with protective gas; the shape of the heating cavity comprises a cylinder, a square, a tube or a sphere; the protective gas comprises one or more of nitrogen, helium and argon.
Preferably, the graphene-based photovoltaic device further comprises a first electrode layer and a second electrode layer, wherein one end of the first electrode layer is electrically connected with the graphene conductive layer, the other end of the first electrode layer is electrically connected with the first conductor, one end of the second electrode layer is electrically connected with the graphene conductive layer, and the other end of the second electrode layer is electrically connected with the second conductor; the first electrode layer and the second electrode layer are metal layers; the thickness of the first electrode layer is 1-50 μm, and the thickness of the second electrode layer is 1-50 μm.
In another aspect, the present invention provides a method for manufacturing a heater, including the steps of:
(1) cleaning and baking the inner wall area of the heating cavity;
(2) preparing a graphene conducting layer attached to the inner wall of the heating cavity in the inner wall area in the step (1);
(3) respectively connecting one ends of a first conductor and a second conductor at different positions of the graphene conducting layer; the other ends of the first conductor and the second conductor extend to the outside of the heating cavity;
(4) the heating chamber is sealed.
Preferably, the preparing of the graphene conductive layer attached to the inner wall of the heating cavity comprises the following steps: one end of the heating cavity is opened and is placed in a high-temperature hydrogen atmosphere furnace, carbon-containing micromolecule gas is introduced into the region of the inner wall of the heating cavity, which is attached with the graphene conducting layer, through a quartz tubule, the reaction temperature is 800-; the thickness of the graphene conductive layer is 0.001-1 μm; the carbon-containing small molecule gas comprises one or more of methane, ethylene and acetylene.
Preferably, the preparing of the graphene conductive layer attached to the inner wall of the heating cavity comprises the following steps: adding water into graphene oxide with the sheet diameter of 5-500 microns and the oxygen content of 20-50% to prepare a dispersion liquid with the solid content of 0.5-3%, coating the dispersion liquid on the inner wall of a heating cavity, baking for 10-60min at 50-150 ℃, placing in a high-temperature hydrogen atmosphere furnace, reacting at the temperature of 400-1000 ℃ for 10-60min, and preparing to obtain a graphene conducting layer; the thickness of the graphene conductive layer is 0.01-10 um.
Preferably, the preparing of the graphene conductive layer attached to the inner wall of the heating cavity comprises the following steps: the graphene slurry is prepared from graphene powder and a temperature-resistant base material, and is coated on the inner wall of the heating cavity to prepare a graphene conducting layer; the mass content of graphene in the graphite slurry is 0.5-10%; the mass content of the temperature-resistant base material is 10-50%; the thickness of the graphene conductive layer is 10-100 um; the temperature-resistant base material comprises one or more of metal oxide, metal carbide, metal nitride and non-metallic material; the non-metallic material comprises one or more of graphite, silicon carbide, silicon dioxide, silicon and silicon nitride.
Preferably, the method for manufacturing a heater described above further includes the following steps: and respectively connecting the first electrode layer and the second electrode layer at different positions of the graphene conducting layer in a metal deposition mode or a metal slurry sintering mode.
Preferably, the first electrode layer and the second electrode layer are respectively connected to the first conductor and the second conductor by hot press forming, laser welding, ultrasonic welding or fusion welding.
Preferably, before the heating cavity is sealed, the inside of the heating cavity is vacuumized or filled with protective gas.
The invention has the beneficial effects that:
the heater provided by the invention comprises a heating cavity, a graphene conducting layer and a graphene conducting layer, wherein the graphene conducting layer is attached to the inner wall of the heating cavity, heat can directly penetrate through the inner wall of the heating cavity, the effect of rapid and uniform heating is realized, and the heat efficiency is greatly improved; the graphene conducting layer is attached to the inner wall of the heating cavity, a self-supporting structure is not needed, the graphene conducting layer is well attached to the inner wall of the heating cavity, no obvious requirement is made on the mechanical strength of the graphene conducting layer, and the manufacturing cost of the heater is reduced; the graphene conducting layer is attached to the inner wall of the heating cavity, the shape of the heating cavity is not limited at all, and a heater in any shape can be realized.
The heating cavity is well sealed, the interior of the heating cavity is vacuum or filled with protective gas, the graphene conducting layer in the heating cavity has the plane resistance of 0.01-1000 omega, can resist the high temperature of 1100 ℃ plus materials at the working temperature of 800 ℃, has the service life of more than 30000h, and can realize the effect of more than 20W/cm2The power density of (d); the heating cavity is isolated from the outside, and the prepared heater can realize good waterproof performance and insulating performance.
Drawings
FIG. 1 is a schematic diagram of a graphene layer without an electrode layer attached to a heating chamber;
FIG. 2 is a schematic diagram of a structure in which a graphene layer containing an electrode layer is attached to a heating chamber;
fig. 3 is a schematic structural view of the conductor on the same side of the heating cavity.
The reference numbers in the drawings of the specification are as follows:
1. a graphene conductive layer; 2. heating the cavity; 3. a first conductor; 4. a second conductor; 5. a first electrode layer; 6. a second electrode layer.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects solved by the present invention more clearly apparent, the present invention is further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
As shown in fig. 1, the present invention provides a heater, which includes a graphene conductive layer 1, a heating cavity 2, a first conductor 3, and a second conductor 4; a first conductor 3 and a second conductor 4 are respectively and electrically connected to different positions of the graphene conductive layer 1, and the first conductor 3 and the second conductor 4 extend to the outside of the heating cavity 2; the graphene conducting layer 1 is attached to the inner wall of the heating cavity 2, and the heating cavity 2 is of a sealing structure.
In some embodiments, the graphene conductive layer 1 is attached to the inner wall of the heating cavity 2, and an independent supporting structure is not required, so that the graphene conductive layer 1 is well attached to the inner wall of the heating cavity 2, the mechanical strength of the graphene conductive layer 1 is not obviously required, the manufacturing cost of the graphene conductive layer is reduced, and the manufacturing cost of heating elements such as a heater is also reduced. Graphite alkene conducting layer 1 is attached to 2 inner walls of heating cavity, and the heat can directly pass the heating cavity inner wall and heat the object of heating chamber contact, and the thermal efficiency promotes by a wide margin, realizes the effect of quick even heating. The graphene conducting layer 1 provided by the invention is attached to the inner wall of the heating cavity 2, the shape of the heating cavity 2 is not limited by the structure, the heating cavity 2 can be manufactured into any shape, for example, the heating cavity 2 can be manufactured into structures with various shapes such as a tubular shape, a square shape, a cylindrical shape and a spherical shape, the graphene conducting layer 1 can be manufactured into various forms such as a plane, an arc surface and a patterning shape, and the prepared heater can also be prepared into various suitable shapes according to the heating requirement; the graphene conductive layer provided by the embodiment is attached to the inner wall of the heating cavity 2, the shape of the heating cavity, the shape of the graphene conductive layer 1 and the shape of the heater are not limited, a user can set any structure suitable for heating objects according to the shape of the heating objects, the heating efficiency can be improved, and the attractive effect can be increased.
In some embodiments, one end of the graphene conductive layer 1 is electrically connected to one end of the first conductor 3, and the other end of the first conductor 3 extends to the outside of the heating cavity 2 and is connected to a power supply device; the other end of the graphene conducting layer 1 is electrically connected with one end of a second conductor 4, and the other end of the second conductor 4 extends to the outside of the heating cavity 2 and is connected with a power supply device; the power is carried the electric energy for graphite alkene conducting layer 1, and graphite alkene conducting layer 1 passes through far infrared radiation with electric energy conversion heat around with the heat, and heat transfer is for heating cavity 2. In the present embodiment, the first conductor 3 and the second conductor 4 are similar to metal wires, and can transmit electric energy.
In the embodiment, the heating cavity 2 is a sealing structure, so that air is isolated, graphene in the graphene conducting layer is prevented from being oxidized, and meanwhile, the temperature resistance of the graphene conducting layer 1 can be greatly improved; the sealing structure of the heating cavity 2 effectively isolates the electrified heating area in the closed cavity, and the prepared heater can realize good waterproof performance and insulating performance.
Graphene has fabulous electric heat conversion efficiency in graphite alkene conducting layer 1 in this embodiment, and graphite alkene conducting layer 1 circular telegram back, graphite alkene can the efficient convert the electric energy into heat energy, according to the heat radiation characteristic of graphite alkene itself, radiates away the heat with modes such as far infrared with heat energy to realize the effect that the electric energy converts heat energy into fast.
The parts of the first conductor 3 and the second conductor 4 extending to the outside of the heating cavity 2 are respectively disposed at two sides of the heating cavity 2, or disposed at the same side of the heating cavity 2, as shown in fig. 3, the parts of the first conductor 3 and the second conductor 4 extending to the outside of the heating cavity 2 are disposed at the same side of the heating cavity 2. The present embodiment does not limit the specific position of the portion extending to the outside of the heating chamber 2.
The interior of the heating cavity 2 is in a vacuum state or is filled with protective gas; the protective gas includes one of nitrogen, helium and argon, and the type of the protective gas is not limited in the invention, so long as the effect of preventing graphene oxidation is achieved. The material of the heating cavity 2 may be quartz, glass, ceramic, etc. which may be common temperature-resistant insulating materials.
The heater further comprises a first electrode layer 5 and a second electrode layer 6, wherein one end of the first electrode layer 5 is electrically connected with the graphene conducting layer 1, the other end of the first electrode layer 5 is electrically connected with the first conductor 3, one end of the second electrode layer 6 is electrically connected with the graphene conducting layer 1, and the other end of the second electrode layer 6 is electrically connected with the second conductor 4; the first electrode layer 5 and the second electrode layer 6 are metal layers; the thickness of the first electrode layer 5 is 1-50 μm, and the thickness of the second electrode layer 6 is 1-50 μm.
In some embodiments, as shown in fig. 2, the heater structure is that two ends of the graphene conductive layer 1 are electrically connected to the first electrode layer 5 and the second electrode layer 6, respectively, the other ends of the first electrode layer 5 and the second electrode layer 6 are electrically connected to one ends of the first conductor 3 and the second conductor 4, respectively, and the other ends of the first conductor 3 and the second conductor 4 extend through the outside of the heating cavity to be connected to the power supply device.
In some embodiments, the first electrode layer 5 and the second electrode layer 6 are formed at two ends of the graphene conductive layer 1 by sintering metal slurry, or the first electrode layer 5 and the second electrode layer 6 are formed at two ends of the graphene conductive layer 1 by metal deposition and electrically connected to the graphene conductive layer 1; wherein the conductive metal is copper, aluminum, molybdenum, silver, iron, etc. The first electrode layer 5 and the second electrode layer 6 are formed as metal layers and have a thickness of 1 to 50 μm. The thickness of the electrode layer is higher than the range value, the thickness of the electrode layer is increased, the corresponding internal resistance is increased, the electric energy consumption is increased, and the electrode layer is easy to fall off in the heating process; the thickness of the electrode layer is lower than the range value, and the electrode layer structure is not easy to form. Electric energy generated by the power supply device is transmitted to the graphene conducting layer 1 through the first conductor, the second conductor, the first electrode layer and the second electrode layer, wherein the first electrode layer and the second electrode layer are mainly used for transmitting the electric energy; the heater may or may not include the first and second electrode layer structures.
The graphene conductive layer 1 can be prepared by carbon micromolecular gas through a chemical vapor deposition method, and comprises the following specific steps: placing a heating cavity 2 with an opening at one end in a high-temperature hydrogen atmosphere furnace, introducing one or more carbon-containing micromolecule gases of methane, ethylene and acetylene into a region of the inner wall of the heating cavity to heat the gas temperature in the heating cavity, and preparing the graphene conducting layer attached to the inner wall of the heating cavity under the conditions that the reaction temperature is 800-1000 ℃ and the reaction time is 10-60min, wherein the thickness of the prepared graphene conducting layer is 0.001-1 mu m.
In some embodiments, in the area where the graphene conductive layer 1 is directly attached to the inner wall of the heating cavity 2, the inner wall of the heating cavity 2 is used as a carrier, the graphene conductive layer 1 is prepared by using a chemical vapor deposition method, and graphene permeates into gaps in the inner wall of the heating cavity 2, and compared with the method that a graphene conductive film is prepared first and then is attached to the inner wall 2 of the heating cavity, the graphene conductive layer 1 is prepared directly on the inner wall of the heating cavity by using the chemical vapor deposition method, so that the adhesion force between the prepared graphene conductive layer 1 and the heating cavity 2 is enhanced, the heat radiation of the graphene conductive layer 1 to the heating cavity 2 and a heating object in contact with the heating cavity 2 is facilitated, and the heat transfer efficiency is improved. The thickness of the graphene conducting layer 1 prepared by the chemical vapor deposition method is 0.001-1 mu m, when the thickness of the graphene conducting layer 1 is higher than 1 mu m, the adhesive force between the graphene conducting layer 1 and the inner wall of the heating cavity 2 is reduced, the graphene conducting layer is easy to crack and fall off in the heating process, and the heat transfer efficiency is reduced.
The graphene conductive layer 1 in the invention can be formed by coating graphene oxide slurry, and the specific steps are as follows: adding water into graphene oxide with the sheet diameter of 5-500 microns and the oxygen content of 20-50% to prepare a dispersion liquid with the solid content of 0.5-3%, coating the dispersion liquid on the inner wall of the heating cavity 2, baking at 50-150 ℃ for 10-60min, and then placing in a high-temperature hydrogen atmosphere furnace, wherein the reaction temperature is 400-1000 ℃ and the reaction time is 10-60min, so as to prepare the graphene conducting layer with the thickness of 0.01-10 microns.
In some embodiments, graphene oxide slurry with a solid content of 0.5-3.0% is prepared, and then the graphene oxide slurry is coated on the inner wall of a heating cavity 2, and a graphene conducting layer 1 is obtained by hydrogen reduction, and by using the method, a dense graphene conducting layer 1 can be formed on the surface of the inner wall of the heating cavity 2, because graphene oxide contains an oxygen-containing functional group, the graphene oxide slurry can be more uniformly dispersed in water, the graphene oxide slurry is coated on the surface of the inner wall of the heating cavity 2, the graphene oxide is uniformly distributed, and then the uniformly and densely distributed graphene conducting layer 1 can be obtained by hydrogen reduction, the uniformly and densely distributed graphene conducting layer 1 is attached to the inner wall of the heating cavity 2, the graphene electrothermal radiation is uniform, the heat is uniformly and rapidly transferred to a heating object through the inner wall of the cavity, and the heat efficiency is improved. The solvent for preparing the graphene oxide slurry is water, the type of the solvent for preparing the graphene oxide slurry is not limited in the invention, and the solvent only needs to be capable of dispersing graphene oxide in the solvent.
The graphene conductive layer 1 in the invention can also be formed by coating graphene slurry, and the specific steps are as follows: the graphene slurry is prepared from graphene powder and a temperature-resistant base material, and the graphene slurry is coated on the inner wall of the heating cavity to prepare the graphene conducting layer with the thickness of 10-100 um. Wherein the graphene mass content in the graphite slurry is 0.5-10%; the mass content of the heat-resistant base material is 10-50 percent; the solvent accounts for 60 to 90 percent. The solvent may be ethanol, butanol, glycol ester, ethyl acetate, but the kind of the solvent is not limited as long as graphene can be dispersed in the solvent. The temperature-resistant base material comprises one or more of metal oxide, metal carbide, metal nitride and non-metallic material; wherein the non-metallic material comprises one or more of graphite, silicon carbide, silicon dioxide, silicon and silicon nitride.
In some embodiments, the temperature-resistant base material provided by the invention is required to have high temperature resistance, and can be well combined with graphene, the graphene slurry is coated on the inner wall of the heating cavity 2, the graphene is uniformly distributed, the graphene powder is combined with the temperature-resistant base material to prepare the graphene conducting layer 1, and after the graphene conducting layer is electrified, the graphene can efficiently convert electric energy into heat energy, and the heat energy is rapidly radiated out in a far infrared ray mode and the like. The thickness of the graphene conducting layer 1 is 10-100 μm, and when the thickness is less than 10 μm, the thickness of the graphene conducting layer is too thin, so that large-scale production and processing are difficult, and the conductivity is difficult to meet the application requirements.
The preparation method for preparing the graphene conducting layer 1 by the three methods is easy to realize and is easy for large-scale production and application; the prepared graphene conducting layer 1 attached to the inner wall of the heating cavity 2 has the plane resistance of 0.01-1000 omega, can resist the high temperature of 800-1100 ℃, can stably work at the temperature of 800 ℃ for a long time, and can realize the temperature of more than 20W/cm2The power density of (a).
The preparation method of the heater comprises the following steps:
the method comprises the following steps: cleaning and baking the inner wall area of the heating cavity;
step two: and preparing the graphene conductive layer 1 attached to the inner wall of the heating cavity 2 by the chemical vapor deposition method, the graphene oxide slurry coating method and the graphene slurry coating method.
Step three: preparing and forming a first electrode layer 5 and a second electrode layer 6 at the edges of two ends of the graphene conducting layer 1 by metal slurry sintering or a metal deposition method; and then the other ends of the first electrode layer 5 and the second electrode layer 6 are electrically connected with one ends of the first conductor 3 and the second conductor 4 through hot press molding, laser welding, ultrasonic welding or fusion welding.
The two ends of the graphene conductive layer 1 may also be selectively not connected to the first electrode layer 5 and the second electrode layer 6, and may be directly electrically connected to one ends of the first conductor 3 and the second conductor 4 by hot press molding, laser welding, ultrasonic welding or fusion welding.
Step four: the other ends of the first conductor 3 and the second conductor 4 penetrate through the heating cavity 2 and extend to the outside of the heating cavity 2, and the contact positions of the first conductor 3 and the second conductor 4 and the heating cavity 2 are required to be sealed.
Step five: the heating chamber 2 is evacuated or filled with a protective gas, and both ends of the heating chamber 2 are completely sealed. The heater provided by the invention can be used as an immersion heater, a dry-burning heater, a surface heating heater and a far infrared heater, and can also be applied to the fields of water heaters, electric boilers, barbecue ovens, baking trays, cooking pans, electric cookers, hot pot heating plates, heaters, industrial ovens, industrial tunnel furnaces and the like.
The present invention will be further illustrated by the following examples.
Example 1
Cleaning and baking the inner wall area of the heating cavity.
The preparation method of the graphene conductive layer 1 attached to the inner wall of the heating cavity 2 comprises the following specific steps: and (2) placing the heating cavity 2 with an opening at one end in a high-temperature hydrogen atmosphere furnace, introducing methane gas into a region where the graphene conducting layer is attached to the inner wall of the heating cavity through a quartz tubule, heating to 800 ℃, and reacting for 60min to obtain the graphene conducting layer 1 with the thickness of 1 micrometer.
The edges of two ends of the graphene conducting layer 1 are sintered by copper slurry to form a first electrode layer 5 and a second electrode layer 6; and then the other ends of the first electrode layer 5 and the second electrode layer 6 are electrically connected with one ends of the first conductor 3 and the second conductor 4 through a hot press molding mode. The other ends of the first conductor 3 and the second conductor 4 penetrate through the heating cavity 2 to extend to the outside of the heating cavity 2, and the contact positions of the first conductor 3 and the second conductor 4 and the heating cavity 2 are sealed. The heating chamber 2 is evacuated and both ends of the heating chamber 2 are completely sealed.
Example 2 to example 5
Examples 2 to 5 are different from example 1 in that the thickness of the conductive layer of graphene produced is different depending on the reaction temperature and the reaction time.
Example 6
Cleaning and baking the inner wall area of the heating cavity.
Adding water into graphene oxide with the sheet diameter of 5um and the oxygen content of 20% to prepare a dispersion liquid with the solid content of 0.5%, coating the dispersion liquid on the inner wall of the heating cavity 2, baking for 60min at 80 ℃, placing in a high-temperature hydrogen atmosphere furnace, reacting at 800 ℃ for 60min, and preparing the graphene conducting layer 1 with the thickness of 5 um.
The edges of two ends of the graphene conducting layer 1 are electrically connected with one ends of the first conductor 3 and the second conductor 4 in an ultrasonic welding mode. The other ends of the first conductor 3 and the second conductor 4 penetrate through the heating cavity 2 to extend to the outside of the heating cavity 2, and the contact positions of the first conductor 3 and the second conductor 4 and the heating cavity 2 are sealed. The inside of the heating chamber 2 is filled with nitrogen gas and both ends of the heating chamber 2 are completely sealed.
Examples 7 to 10
Example 7-example 10 differs from example 6 in baking time, reaction time, temperature, and thickness of the graphene conductive layer 1; the graphene oxide slurry has different sheet diameters and different oxygen contents, and the graphene oxide slurry has different solid contents.
Example 11
Cleaning and baking the inner wall area of the heating cavity.
Preparing graphene powder with the mass content of 0.5%, silicon carbide temperature-resistant base material with the mass content of 10% and ethanol solvent with the mass content of 89.5% to form uniformly dispersed graphene slurry; and coating the graphene slurry on the inner wall of the heating cavity 2 to prepare the graphene conducting layer with the thickness of 10 microns.
The edges of two ends of the graphene conducting layer 1 are sintered by aluminum paste to form a first electrode layer 5 and a second electrode layer 6; then, the other ends of the first electrode layer 5 and the second electrode layer 6 are electrically connected to one ends of the first conductor 3 and the second conductor 4 by ultrasonic welding. The other ends of the first conductor 3 and the second conductor 4 penetrate through the heating cavity 2 to extend to the outside of the heating cavity 2, and the contact positions of the first conductor 3 and the second conductor 4 and the heating cavity 2 are sealed. The inside of the heating chamber 2 is filled with helium gas and both ends of the heating chamber 2 are completely sealed.
Example 12
Cleaning and baking the inner wall area of the heating cavity.
Preparing graphene powder with the mass content of 6%, silicon dioxide temperature-resistant base material with the mass content of 30% and butanol solvent with the mass content of 64% to form uniformly dispersed graphene slurry; and coating the graphene slurry on the inner wall of the heating cavity 2 to prepare the graphene conducting layer with the thickness of 50 microns.
The edges of two ends of the graphene conducting layer 1 are sintered by iron slurry to form a first electrode layer 5 and a second electrode layer 6; then, the other ends of the first electrode layer 5 and the second electrode layer 6 are electrically connected to one ends of the first conductor 3 and the second conductor 4 by fusion welding. The other ends of the first conductor 3 and the second conductor 4 penetrate through the heating cavity 2 to extend to the outside of the heating cavity 2, and the contact positions of the first conductor 3 and the second conductor 4 and the heating cavity 2 are sealed. Argon gas is filled in the heating chamber 2 and both ends of the heating chamber 2 are completely sealed.
Example 13
Cleaning and baking the inner wall area of the heating cavity.
Preparing graphene powder with the mass content of 10%, silicon nitride temperature-resistant base material with the mass content of 50% and glycol ester solvent with the mass content of 40% to form uniformly dispersed graphene slurry; and coating the graphene slurry on the inner wall of the heating cavity 2 to prepare the graphene conducting layer with the thickness of 100 microns.
The edges of two ends of the graphene conducting layer 1 are sintered by molybdenum slurry to form a first electrode layer 5 and a second electrode layer 6; then, the other ends of the first electrode layer 5 and the second electrode layer 6 are electrically connected to one ends of the first conductor 3 and the second conductor 4 by laser welding. The other ends of the first conductor 3 and the second conductor 4 penetrate through the heating cavity 2 to extend to the outside of the heating cavity 2, and the contact positions of the first conductor 3 and the second conductor 4 and the heating cavity 2 are sealed. The heating chamber 2 is evacuated and both ends of the heating chamber 2 are completely sealed.
Comparative example 1
Cleaning and baking the inner wall area of the heating cavity.
The preparation method of the graphene conductive layer 1 attached to the inner wall of the heating cavity 2 comprises the following specific steps: and (2) placing the heating cavity 2 with an opening at one end in a high-temperature hydrogen atmosphere furnace, introducing methane gas into a region where the graphene conducting layer is attached to the inner wall of the heating cavity through a quartz tubule, heating to 800 ℃, and reacting for 60min to obtain the graphene conducting layer 1 with the thickness of 0.01 mu m.
The edges of two ends of the graphene conducting layer 1 are sintered by copper slurry to form a first electrode layer 5 and a second electrode layer 6; and then the other ends of the first electrode layer 5 and the second electrode layer 6 are electrically connected with one ends of the first conductor 3 and the second conductor 4 through a hot press molding mode. The other ends of the first conductor 3 and the second conductor 4 penetrate through the heating cavity 2 to extend to the outside of the heating cavity 2, and the contact positions of the first conductor 3 and the second conductor 4 and the heating cavity 2 are sealed.
The heating cavity is directly sealed without vacuum pumping or protective gas filling operation.
Comparative example 2
Adding water into graphene oxide with the sheet diameter of 5 micrometers and the oxygen content of 20% to prepare a dispersion liquid with the solid content of 0.5%, coating the dispersion liquid on a release film, baking for 60min at 80 ℃, stripping the graphene oxide sheet from the release film to obtain a graphene oxide sheet with the thickness of 50 micrometers, placing the graphene oxide sheet in a high-temperature hydrogen atmosphere furnace, and reacting at the temperature of 800 ℃ for 60min to prepare the graphene conducting layer with the thickness of 5 micrometers.
The edges of two ends of the graphene conducting layer 1 are electrically connected with one ends of the first conductor 3 and the second conductor 4 in an ultrasonic welding mode. The other ends of the first conductor 3 and the second conductor 4 penetrate through the heating cavity 2 to extend to the outside of the heating cavity 2, and the contact positions of the first conductor 3 and the second conductor 4 and the heating cavity 2 are sealed. The graphene conductive layer 1 is suspended in the heating cavity.
The inside of the heating chamber 2 is filled with nitrogen gas and both ends of the heating chamber 2 are completely sealed.
Comparative example 3
Preparing graphene powder with the mass content of 0.5%, silicon carbide temperature-resistant base material with the mass content of 10% and ethanol solvent with the mass content of 89.5% to form uniformly dispersed graphene slurry; and coating the graphene slurry on a release film, drying, peeling and rolling to obtain the graphene conducting layer with the thickness of 10 microns.
The edges of two ends of the graphene conducting layer 1 are sintered by aluminum paste to form a first electrode layer 5 and a second electrode layer 6; then, the other ends of the first electrode layer 5 and the second electrode layer 6 are electrically connected to one ends of the first conductor 3 and the second conductor 4 by ultrasonic welding. The other ends of the first conductor 3 and the second conductor 4 penetrate through the heating cavity 2 to extend to the outside of the heating cavity 2, and the contact positions of the first conductor 3 and the second conductor 4 and the heating cavity 2 are sealed. The graphene conducting layer is suspended in the heating cavity.
The inside of the heating chamber 2 is filled with helium gas and both ends of the heating chamber 2 are completely sealed.
Table 1 examples 7-10 graphene oxide slurries processing parameters
Figure BDA0003256367040000121
Table 2 examples 1-13, comparative examples 1-3 graphene conductive layer test performance data
Figure BDA0003256367040000122
Figure BDA0003256367040000131
And (3) coating the graphene slurry on a release film, drying, peeling and rolling to prepare a 10-micrometer-thick graphene conducting layer, and testing performance data shows that after the working temperature of the graphene conducting layer prepared by the method in the comparative example 3 exceeds 300 ℃, the graphene conducting layer is broken due to obvious uneven thermal expansion, loses a heating function and cannot normally work at 800 ℃.
As can be seen from comparison of examples 1-5 with comparative example 1 in Table 2, the heater prepared by the method has poor performance data such as plane resistance, power density and the like, although the other preparation methods are the same, the heating cavity is directly sealed without vacuum pumping or is filled with protective gas; comparing the comparative example 2 with the examples 6-10, it can be seen that the graphene conductive layer directly coated on the inner wall of the heating cavity has better plane resistance, power density and working temperature data; compared with the embodiments 11 to 13, in the method of the present invention, compared with the method of the embodiments 11 to 13, the tolerance temperature of the graphene conductive layer prepared by the method of the embodiments 11 to 13 is higher, the working life of 800 ℃ is longer than 30000h, which is much longer than 1000h in the comparative example 3. The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.

Claims (10)

1. The utility model provides a heater, its characterized in that includes heating cavity, graphite alkene conducting layer, first conductor and second conductor, graphite alkene conducting layer adhere to heating cavity inner wall, first conductor with the second conductor electricity respectively connect in the different positions of graphite alkene conducting layer, first conductor with the second conductor extends to the heating cavity outside, the heating cavity is seal structure.
2. The heater of claim 1, wherein said first conductor and said second conductor extend to an exterior portion of said heating chamber on either side of said heating chamber or on the same side of said heating chamber; the interior of the heating cavity is in a vacuum state or is filled with protective gas; the shape of the heating cavity comprises a cylinder, a square, a tube or a sphere; the protective gas comprises one or more of nitrogen, helium and argon.
3. The heater according to claim 1, further comprising a first electrode layer and a second electrode layer, wherein one end of the first electrode layer is electrically connected to the graphene conductive layer, the other end of the first electrode layer is electrically connected to the first conductor, one end of the second electrode layer is electrically connected to the graphene conductive layer, and the other end of the second electrode layer is electrically connected to the second conductor; the first electrode layer and the second electrode layer are metal layers; the thickness of the first electrode layer is 1-50 μm, and the thickness of the second electrode layer is 1-50 μm.
4. A method of manufacturing a heater according to any one of claims 1 to 3, comprising the steps of:
(1) cleaning and baking the inner wall area of the heating cavity;
(2) preparing a graphene conducting layer attached to the inner wall of the heating cavity in the inner wall area in the step (1);
(3) respectively connecting one ends of a first conductor and a second conductor at different positions of the graphene conducting layer; the other ends of the first conductor and the second conductor extend to the outside of the heating cavity;
(4) the heating chamber is sealed.
5. The method for preparing the heater according to claim 4, wherein the step of preparing the graphene conductive layer attached to the inner wall of the heating cavity comprises the following steps: one end of the heating cavity is opened and is placed in a high-temperature hydrogen atmosphere furnace, carbon-containing micromolecule gas is introduced into the region of the inner wall of the heating cavity, which is attached with the graphene conducting layer, through a quartz tubule, the reaction temperature is 800-; the thickness of the graphene conductive layer is 0.001-1 μm; the carbon-containing small molecule gas comprises one or more of methane, ethylene and acetylene.
6. The method for preparing the heater according to claim 4, wherein the step of preparing the graphene conductive layer attached to the inner wall of the heating cavity comprises the following steps: adding water into graphene oxide with the sheet diameter of 5-500 microns and the oxygen content of 20-50% to prepare a dispersion liquid with the solid content of 0.5-3%, coating the dispersion liquid on the inner wall of a heating cavity, baking for 10-60min at 50-150 ℃, placing in a high-temperature hydrogen atmosphere furnace, reacting at the temperature of 400-1000 ℃ for 10-60min, and preparing to obtain a graphene conducting layer; the thickness of the graphene conductive layer is 0.01-10 um.
7. The method for preparing the heater according to claim 4, wherein the step of preparing the graphene conductive layer attached to the inner wall of the heating cavity comprises the following steps: the graphene slurry is prepared from graphene powder and a temperature-resistant base material, and is coated on the inner wall of the heating cavity to prepare a graphene conducting layer; the mass content of graphene in the graphite slurry is 0.5-10%; the mass content of the temperature-resistant base material is 10-50%; the thickness of the graphene conductive layer is 10-100 um; the temperature-resistant base material comprises one or more of metal oxide, metal carbide, metal nitride and non-metallic material; the non-metallic material comprises one or more of graphite, silicon carbide, silicon dioxide, silicon and silicon nitride.
8. The method of claim 4, further comprising the steps of: and respectively connecting the first electrode layer and the second electrode layer at different positions of the graphene conducting layer in a metal deposition mode or a metal slurry sintering mode.
9. The method of claim 8, wherein the first electrode layer and the second electrode layer are connected to the first conductor and the second conductor by hot press forming, laser welding, ultrasonic welding or fusion welding, respectively.
10. The method of claim 9, wherein the heating chamber is evacuated or filled with a protective gas before the heating chamber is sealed.
CN202111061001.3A 2021-09-10 2021-09-10 Heater and preparation method thereof Pending CN113840400A (en)

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